Hindawi Publishing Corporation
Journal of Nanomaterials
Volume 2010, Article ID 203756, 7 pages
doi:10.1155/2010/203756
Research Article
Template-Based Electrochemically Controlled Growth of
Segmented Multimetal Nanorods
Mee Rahn Kim, Dong Ki Lee, and Du-Jeon Jang
School of Chemistry, Seoul National University, NS60, Seoul 151-742, Republic of Korea
Correspondence should be addressed to Du-Jeon Jang, djjang@snu.ac.kr
Received 20 September 2010; Revised 19 November 2010; Accepted 10 December 2010
Academic Editor: Do Kim
Copyright © 2010 Mee Rahn Kim et al. This is an open access article distributed under the Creative Commons Attribution License,
which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
Multisegmented one-dimensional nanostructures composed of gold, copper, and nickel have been fabricated by depositing metals
electrochemically in the pores of anodic aluminum oxide (AAO) templates. The electrodeposition process has been carried out
using a direct current in a two-electrode electrochemical cell, where a silver-evaporated AAO membrane and a platinum plate have
served as a working electrode and a counter electrode, respectively. The striped multimetal rods with an average diameter of about
300 nm have tunable lengths ranging from a few hundred nanometers to a few micrometers. The lengths and the sequence of metal
segments in a striped rod can be tailored readily by controlling the durations of electrodeposition and the order of electroplating
solutions, respectively.
1. Introduction
Nanostructured materials have been extensively developed
in fabrication methods and modified properties, and application ranges from fundamental science to industrial technology [1–9]. Metal nanoparticles are well known for
their optical, electrical, thermal, catalytic, and magnetic
properties as well as for biological interactions between
some noble metals and biomolecules [10–15]. Especially,
one-dimensional metallic nanostructures such as nanorods,
nanowires, and nanotubes exhibit some advantages associated with their anisotropic architecture and allow to be
employed as nanometer-scaled electronic devices and optoelectronic devices [15–17]. Due to their attractive potential
in the miniaturization of devices and in the usage of bioanalysis, tremendous research efforts have been dedicated to their
fabrication and modification [18–25]. Heterostructured
metallic nanorods have been fabricated by many research
groups because they can be used as electrocatalysts or
nanobarcodes. For example, hybrid nanorods composed of
electrocatalytically active metals such as platinum and nickel
can have their maximum catalytic effects [24–26]. When
the body of a metallic nanorod comprises longitudinally
segmented metal sections, the heterostructured nanorod can
be employed as a nanometer-scaled barcode [15, 24, 27].
The conventional methods of preparing one-dimensional
metallic nanostructures are nanolithography and electrochemical deposition [28–32]. In particular, the electrochemical method has attracted much attention owing to its low
cost, operation simplicity, and capability to deposit metallic
materials into nanopores such as anodic aluminum oxide
(AAO) membranes and polycarbonate membranes. AAO
membranes have been easily and extensively employed not
only as templates to fabricate one-dimensional nanostructures of wires and tubes, but also as masters to prepare
ordered arrays of metal nanorings and regularly structured
nanotextures [29–37]. AAO membranes are made by oxidizing aluminum sheets anodically in solutions of sulfuric,
oxalic, and phosphoric acids, and they possess diverse
advantages to be employed as templates [21, 32–34, 38].
First of all, they have uniform pores and parallel channels
of large domains. Second, the diameters and lengths of their
pores can be controlled easily and tailored finely. Third, AAO
membranes offer a high thermal and mechanical stability,
and they are chemically and thermally inert during the
deposition of metals in the pores.
We have fabricated striped multimetal nanorods by
electrodepositing three different metals of gold, copper, and
nickel sequentially in the pores of AAO templates. A directcurrent (DC) electrodeposition process has been carried
2
Journal of Nanomaterials
Ag
evaporation
Au
deposition
Cu deposition
Au
Cu
Ni
Au
deposition
deposition
Au
depositions
AAO
dissolution
Figure 1: Schematically illustrated fabrication procedures of striped multimetal nanorods.
out in a two-electrode electrochemical cell system using a
silver-baked AAO membrane as a working electrode and a
platinum plate as a counter electrode. We will show that the
lengths of metal segments in a striped rod, as well as the
total length of the rod, can be tuned well by controlling the
durations of electrodeposition.
2. Materials and Methods
2.1. Materials. The electroplating solutions of gold (technical gold 410), copper (technical copper PR), and nickel
(high-speed nickel-sulfate process) were obtained from
Hantech PMC. AAO membranes having the pore diameter
of ∼200 nm were purchased from Whatman International,
and silver shots (99.999%) were from Sigma-Aldrich. For
the preparation of a conductive AAO membrane, while an
AAO membrane was placed on the holder of a thermal
vacuum evaporator (Ultimate Vacuum, MHS-1800), silver
shots were loaded on a tungsten boat and evaporated in
a vacuum condition of 10−5 torr on the backside of the
AAO membrane to have silver film thickness of 400 nm. The
silver-evaporated AAO membrane was served as a working
electrode of 0.5 cm2 while a platinum plate was employed as
a counter electrode of 1.5 cm2 . For the preparation of singlecomponent metal nanorods, gold was electrodeposited at
the anodic voltage of DC 4 V for 40 min under sonication
at 45◦ C, nickel was at the anodic voltage of DC 3 V for
5 min under sonication at 45◦ C, and copper was at the
anodic voltage of DC 2 V for 5 min at room temperature.
For the fabrication of multimetal nanorods, gold and nickel
metal segments were electrodeposited at the anodic voltage
of DC 3 V under sonication at 45◦ C for 20 min and for
5 min, respectively, whereas copper was electrodeposited at
the anodic voltage of DC 2 V at room temperature for
3 min. Each electrochemical deposition step requires the
AAO membrane and the electrodeposition cell to be rinsed
out completely. After finishing all the electrodeposition
steps, we washed the specimen with water and dried it
at 50◦ C. Free-standing metallic rods on a silver film were
isolated by dissolving the AAO templates in 1 M NaOH for
1 h, while multimetal rods dispersed in a solution were
prepared by removing the silver film of the specimen in a
12 M HCl solution for 30 s and by dissolving AAO templates
subsequently in 1 M NaOH for 1 h.
2.2. Methods. Field-emission scanning electron microscopy
(FESEM) images, energy-dispersive X-ray (EDX) spectra,
and EDX elemental distribution maps were obtained with a
microscope (JEOL, JSM-6700F) attached to a CCD camera
as the detector. Reflectance spectra were measured using a
UV/vis reflectance spectrometer (StellarNet, EPP2000C UVVIS).
3. Results and Discussion
Figure 1 depicts a process flowchart for the fabrication
of multimetal nanorods in a two-electrode cell system.
After depositing silver thermally on the backsides of AAO
membranes, we deposited three different metals electrochemically in the pores of the AAO membranes. At this stage,
the electrochemical reduction of gold, copper, and nickel
in electroplating solutions was carried out sequentially to
prepare striped multimetal nanorods. The lengths of metal
rods and the sequence of multimetal segments could be
tuned easily by controlling the durations of electrodeposition
and the order of electroplating solutions, respectively. Only
the alumina membrane was removed after electrodeposition
from the specimen to prepare free-standing rod structures,
whereas both the alumina membrane and the silver film were
removed from the specimen to prepare striped-metal rods
dispersed in a solution. Single-component metal nanorods
Journal of Nanomaterials
3
2 µm
2 µm
2 µm
Cu
Pt
Au
Pt
Ni
Pt
Au
Pt Pt Pt
Pt Pt Pt
0
1
2
3
4
5
0
1
2
3
4
5
0
1
2
3
(keV)
(keV)
(keV)
(a)
(b)
(c)
4
5
Figure 2: FESEM top-view images (top) and EDX spectra (bottom) of free-standing nanorods of gold (a), copper (b), and nickel (c) after
removal of AAO templates by treatment with a 1.0 M NaOH solution for 1 h at room temperature.
1.2
Absorbance (OD)
1
0.8
0.6
0.4
0.2
0
300
400
500
600
700
800
Wavelength (nm)
Figure 3: UV/vis reflectance spectra of the free-standing nanorods
of gold (yellow), copper (blue), and nickel (green).
were fabricated by following the same above procedure in a
metal electroplating solution.
Figure 2 shows that highly dense rod arrays of three
different single-component metals are free-standing on Ag
films. Each single-component metal nanorod array is well
constructed, indicating that metal ions in an electroplating
solution are introduced readily and reduced electrochemically in the nanopores of an AAO membrane. The elemental
compositions of gold, copper, and nickel nanorods are
evidenced by the EDX spectra of Figure 2 (where platinum
also appears owing to contamination during Pt sputtering for
FESEM measurements). The average diameters of produced
gold, copper, and nickel rods are 300 ± 35, 383 ± 43, and
374 ± 40 nm, respectively, although the pore diameters of
employed AAO membranes were ∼200 nm. The average
diameters of rods are different from one another depending
on metals, and they are larger than the pore diameters of the
employed templates. The templates of AAO membranes can
be dissolved in strongly acidic or basic solutions [39, 40].
Because the electroplating solutions for the fabrication of
metal rods are strongly acidic or basic, the walls of the AAO
membranes were dissolved to some extent by electroplating
solutions during electrodeposition. Thus, the diameters of
metal nanorods produced in the templates were larger than
the pore diameters of the original templates. We consider
that the diameter of a nanorod increases with time because
the AAO wall surrounding the rod dissolves slowly during
electrodeposition. The pHs of the electroplating solutions
of gold, copper, and nickel are 10, 3, and 4, respectively.
In other words, the electroplating solutions of copper and
nickel are acidic whereas the gold electroplating solution
is basic. Thus, the copper and the nickel electroplating
4
Journal of Nanomaterials
Element
Weight %
Atomic %
OK
21
47.3
Al K
22.7
30.2
Cu L
31.9
18
Pt M
10.7
2
Au M
13.7
2.5
Totals
100
100
O Cu
Au
Pt
Al
Au
Pt
Pt
2 µm
0
1
2
3
4
5
(keV)
(a)
(b)
Figure 4: FESEM image (a) and EDX data (b) of Au-Cu-Au nanorods embedded in an AAO membrane.
2 µm
2 µm
10 µm
(a)
(b)
Au
Cu
Ni
Au
Cu
Ni
Au
Cu
Ni
(c)
(d)
(e)
Figure 5: Illustrations (a), FESEM images (b), and EDX elemental distribution maps ((c), (d), and (e)) of Au-Cu-Au-Ni-Au (top), Au-CuAu-Ni-Au-Ni-Au (middle), and Au-Ni-Au-Cu-Au-Ni-Au nanorods (bottom) embedded in AAO membranes. Yellow, green, and blue colors
in the illustrations denote gold, nickel, and copper, respectively.
solutions made the pore diameters of templates larger than
the gold electroplating solution did, regardless of the dipping
time during electrodeposition. The diameter of a segmented
multimetal nanorod is considered to be not uniform: it may
be the largest in the segment of copper and the smallest in
the segment of gold.
The reflectance spectra of free-standing single-component metal nanorods in Figure 3 are very similar to the
wavelength-dependent reflectance spectra of the respectively
used bulk metals [14, 15] because the sizes of metal rods
are too large to show quantum confinement effects in
absorption. The absorption bands of gold and copper rods
Journal of Nanomaterials
have the maxima at 490 and 530 nm, respectively, whereas
the absorption band of nickel rods has the maximum around
500 nm. Nevertheless, the reflectance spectra of free-standing
metal nanorods in Figure 3 show the absorption characters of
constituent metals well.
The FESEM image of Figure 4 indicates that multisegment nanorods of Au-Cu-Au have been well constructed
along the channels of an AAO membrane. The compositemetal nanorods have been fabricated based on the same
technique used for the preparation of single-component
rods of gold, copper, and nickel. Multimetal rods in the
channels have similar lengths with no cracks generated
from damages at interfaces between gold and copper segments. Although gold segments and copper segments are
not distinguished in the FESEM image, the EDX data
demonstrate that the multi-segment rods consist of gold and
copper. Two metal components of the multimetal rods were
not alloyed because the construction of gold and copper
segments by electrochemical deposition was carried out
sequentially in different baths. The elements of aluminum
and oxygen originated from the templates because AuCu-Au nanorods were embedded in an AAO membrane
whereas platinum resulted from Pt sputtering for the FESEM
measurement.
Figure 5 designates that diverse segments of multimetal nanorods have been fabricated by the sequential
electrodeposition of gold, copper, and nickel metals. The
FESEM images of hybrid metal rods embedded in AAO
membranes show that the gold segments are contrastively
brighter than the segments of copper or nickel. Multistriped metal nanorods of Au-Cu-Au-Ni-Au and Au-Cu-AuNi-Au-Ni-Au have lengths of 6.6 and 9.1 µm, respectively.
The EDX elemental distribution maps, corresponding to the
FESEM images well, indicate that the individual segments
of gold, copper, and nickel can be distinguishable in the
multi-striped metal rods embedded in the AAO templates.
Because the metal rods have the similar heights and exist
in the templates, the segment arrays of each metal look like
horizontal elemental bands. The EDX elemental distribution
maps match well with the illustrations and FESEM images of
striped-metal nanorods.
The EDX elemental distribution maps of Au-Cu-Au-NiAu nanorods (top row in Figure 5) show three horizontal
gold bands and one horizontal copper band clearly. The elemental map of nickel, however, does not show any noticeable
horizontal elemental band because, compared with the gold
and copper, nickel has a low electron density. The interval
between the first and the second horizontal gold bands from
the bottom in the map can overlap to the horizontal copper
band in the map, indicating that the striped multimetal
rods are composed of metal segments. We can estimate the
lengths of the respective metal segments of gold, copper, and
nickel from obtained elemental distribution maps although
the elemental distribution map of nickel is lacking in
information. The estimated length of each gold segment is
1.0 µm whereas that of the copper segment, estimated by the
gap between two horizontal gold bands from the bottom, is
2.0 µm. In addition, the length of the nickel segment having a
featureless elemental intensity can be estimated as 1.5 µm via
5
estimating the interval between two horizontal gold bands
in the map. The metal height sum of 6.5 µm corresponds
adequately to the measured total length of 6.6 µm for the
Au-Cu-Au-Ni-Au rod. The elemental distribution maps of
Au-Cu-Au-Ni-Au-Ni-Au nanorods (middle row in Figure 5)
show four horizontal gold bands and one horizontal copper
band. The horizontal copper band overlaps with the interval
between two horizontal gold bands from the bottom in the
map. We can estimate that the added total length of the
rod is 9.0 µm, which accords with the measured value of
9.1 µm. The bottom row of Figure 5 shows that the long
striped-metal rods of Au-Ni-Au-Cu-Au-Ni-Au have been
also deposited electrochemically well at the same conditions,
except for the quadruply elongated electrodeposition time
of nickel. This implies that the lengths and orders of several
metal segments can be controlled readily in order to fabricate
striped-metal nanorods appropriate for applications. The
length of the nickel segment was estimated to be 8 µm, and
the segment-length sum of 22 µm was found to be similar to
the measured length of 25 µm.
4. Conclusion
We have fabricated multi-segmented one-dimensional
nanostructures composed of gold, copper, and nickel by
depositing metals electrochemically in the pores of AAO
templates. The electrodeposition process was carried out
using DC in a two-electrode electrochemical cell, where a
silver-evaporated AAO membrane and a platinum plate were
employed as a working electrode and a counter electrode,
respectively. The lengths of the striped multimetal rods
with an average diameter of about 300 nm have been
adjusted appropriately from a few hundred nanometers
to a few micrometers by controlling the durations of
electrodeposition. On the other hand, the sequence of metal
segments in a striped nanorod was regulated by changing
electroplating solutions during electrodeposition.
Acknowledgments
This work was supported by research grants through the
National Research Foundation of Korea (NRF) funded by
the Ministry of Education, Science, and Technology (20090082846 and 2010-0015806). D.-J. Jang is thankful to the SRC
program of NRF (R11-2007-012-01002-0) and M. R. Kim
acknowledges the BK21 scholarship.
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